Process of manufacturing lubricating-oils



UNITED STATES PATENT OFFICE.

HELMUT KLEvEn, LUDWIG CARL LAUTENSCHLAGER. AND OSWALD HELMUTH GGHRING, or KARLSRUHE, Grimm; ASSIGNORS, BY MESNE ASSIGIL, MENTS, 'ro THE CHEMICAL FOUNDATION, 11m, A CORPORATION or DELA;

Patented Aug. 24, 1920.

WARE.

PROCESS OF MANUFACTURING'LUBRIGATING-OILS.

1 350 814 Specification of Letters Patent.

No Drawing. Application filed February 14, 1916. Serial No. 78,311.

To all whom it may concern Be it known that we, HELMUT KLEVER, LUDWIG CARL LAUTENsCHLAGER, and OSWALD HELMUTH Gormmo, Ph. D., chemists, citizens of the German Empire, residing at Karlsruhe, in the Grand Duchy of Baden, Germany, have invented certain new and useful Improvements in Processes of Manufactu ring Lubricating-Oils, of which the following is a specification.

It is well known that coal tar oils yield lubricating agents of inferior quality. In accordance with our invention-however the viscosity of coal tar oils is increased and it is possible to compensate the lack in ad'- hesive qualities by the effects of an increase in toughness. In accordance with our invention we have discovered that the viscosity of coal tar oils may be increased by the condensation and polymerization of compounds contained therein and capable of such reaction. These points are produced by heating the oils for some time at high temperatures. The oils are thus converted into valuable pressure lubricating oils. This is due to the fact that coal tar oils, particularly the anthracene oils and the naphthalene oils, and the distillation products of coal tar pitch, containing bases and phenols of high molecular weight are capable of condensation by prolonged heating. Some of the bases liberate ammonia, while the phenols liberate water. This heatin of the coal tar oils is preferably effecte under pressure or by allowing the condensed vapors to flow back, so as to avoid losses. The oils obtained are the more viscous or less liquid, the longer they have been heated and the higher the temperature employed. By increasing the amount of air admitted during the heating-process, the oils will be converted into pitch. Air should therefore be excluded as much as possible from the reactions going on during the heating process.

The admission of a very limited amount of air, which is governed by the origin and the composition of the oils employed and which has to be ascertained by a preliminary test, promotes the reactions mentioned. The admission of air must be adjusted in such a manner that it does not convert the flammable components are then distilled off at their respective boiling points, a residue is obtained which constitutes a lubricating oil of high viscosity. In this manner even the lighter distillation products of coal tar are suitable for treatment by this process.

Inasmuch as the thickening of the oil is chiefly due to the condensation of bases and of phenols, it is obvious that coal tar oils can be particularly adapted for the process of our invention by increasing the amount of bases and phenols therein according to well known processes or by adding such components includin those which may be obtained from tar 011s of other origin, as

for instance from wood tar. As a matter of fact the coal tar oils which have been enriched in bases and phenols in accordance with well known processes, show the thickening efli'ect 'of the process of our invention in a particularly marked manner.

The bases and phenols mentioned may also be heated by themselves in accordance with the present process, masses similar to.

petroleum pitch being obtained thereby which may be added to the coal tar oils in order to produce lubricants of high viscosity. In a general way the productivity of our process may be improved by inspissating part of the coal tar oils to be treated, to a very high degree by itself. A product of the desired average viscosity may be obtained by the addition of the inspissated product to oils not so treated.

The processes of condensation and polymerization described may be assisted by the addition of small amounts of catalyzers, for instance one to two per cent. thereof. Of such catalyzers we may mention, Florida earth, kieselguhr,animal charcoal, powdered graphite, chlorids of metals, such as the chlorids of aluminium, zinc, iron, cadmium, copper proto-chlorid and the like, also metallic powder, powdered metal oXids and metal hydroxids, such as those of iron, nickel, cobalt, chromium, aluminium, zinc, copper, lead and the like, or the oxids and hydroxids of the alkali and alkaline earth metals.

By the treatment in accordance with our process the congealing point of the final products is improved as a general rule as compared with those of the crude material. The crystalline bodies, such as anthracene, indene, picene and the like which separate out when the coal tar oils are cooledand cause so much trouble, are considerably less noticeable in the oils treated according to our invention. In accordance with the origin and the composition of the coal tar oils employed the heating may be carried out in such a manner as to avoid suchseparations entirely, the oils solidifying homogeneously.

When it is desired to produce oils of very low congealing point it is preferable to remove the products which crystallize most easily, from the crude oils in accordance with known processes, by distillation for instance of the fractions containing the precipitating bodies or by keeping them for a long time at a low temperature, and then submitting the oils to suction or to centrifugal action. These 0 erations are likewise applicable to the inspissated oils.

The oils obtained according to our process are especially characterized by their very faint odor as compared with the original oils. They are eminently adapted for all lubricatin purposes particularly for lubrication un er pressure.

Examples.

\ yield is substantiall quantitative. During solidification consi erably less crystalline separations are noticed than in the crude oil.

II. Heat 200 pounds anthracene oil II fat oil) ofa viscosit of about 19 degrees ngler (+20 degrees ina pressure boiler for about 24 hours at about 380 degrees C.

A high viscid oil is obtained, possessin the viscosity of aboutv 10 to 15 degrees at +50 de rees C.

so By di ssolving 132 pounds of this highly viscid oil in 68 pounds of the untreated crude oil, an oil having the viscosit of about 55 to degr. E. (+20 degrees C is obtained. a

55 III. Heat 200 pounds of fat oil of a viscosity of about 19 degrees Engler (20 degrees C.) under pressure at about 420 degrees C. from 7 to 10hours. A resin-like tough mass is obtained which is dissolved in an equal amount of anthracene oil I from 70 which the naphthalene fractions have been removed resulting in an oil of the viscosity 90 to 100 degrees Engler (20 degrees C.)..

IV. 196 to 198 pounds of the naphthalene fraction of the tar boiling point 200 to 280 degr. C. (measured in the vapors) and of a viscosity of about 1.5 degr. Engler, are heated for-24 hours at 350 degrees C. in a pressure boiler with 2 to 4 pounds of iron powder or oxid of iron powder. After cooling the product is distilled until the boiling point 280 degrees C. (determinedinthe vapors) has been'reached. There remain about 50 to 56 pounds of an oil possessing the viscosit of about degrees Engler (20 de r. v

y distilling off 72 per Cent, of'the fractions of lowerboiling point from the untreatedoriginal pil, a residue of about 5 to 7 degr. Engler (20 degrees C.) was obtained.

V. 196 to 198 pounds of dehydrated anthracene oil II (fat oil) of viscosity about 19 degrees E. (20 degrees C.) are heated for 24 hours with the exclusion of air under a reflux conden'sen with 2 to 4 pounds of powdered iron or oxid of iron. The boiling point of the liquid is about 315 C. atthe beginning of the boiling and rises during the boiling to about 325 degrees C. An oil in substantially quantitative proportions is,100 produced possessing the viscosity of about 40 to 50 degrees E. at +20 degrees C. By allowing the boiling to continue for 48 hours, an oil results having at +20 (3., a

viscosity of about 50 to 60 degrees Engler and at +50 C. the viscosity of 4.5 to 5.0 degr. E. The oil produced under these conditions is lighter colored than the oils obtained in accordance with the preceding examples. It is clearly soluble in benzol and x yilol and with faint fluorescence in mineral 01 s.

VI. 196 to 198 pounds dehydrated anthracene oil II fat oil) of a viscosity of about 19 degrees ngler (+20 C.) are boiled under a reflux condenser for 24 hours with, from 2 to 4 pounds of iron powder or powdered oxid of iron. :According to the 'nature of the oil employed air is admitted tov the boiling oil during a certain time which has been ascertained by a previous test.

The lower. the boiling point of the liquid the longerthe air maybe allowed-to remain in contact with the oil as a general rule, without the formation of pitch-like .byproducts which are insoluble in benzol. The viscosity of the final product treated with air, is considerably higher than that of an oil boiled with the exclusion of air. By using the anthracene oil mentioned and comliberation of ammonia and of water.

pressure within and without the boiler, a

viscosity of about 50 to degrees Engler (+20 degr. C.) was produced. 2

VII. 186 pounds of anthracene oil II (fat oil) of a viscosity of about 19 degr. E. (+20 C.) are boiled with 10 pounds phenol from wood tar from which the fractions boiling up to about 280 degrees C. had been removed, and with 4 pounds of iron powderwith the exclusion of air under a reflux condenser for 24 hours,- resulting in a lubricating oil which possesses the viscosity of about 50 to degrees Engler (+20 C.)

VIII. About 42 pounds of bases and 24 pounds of phenol obtained from anthracene oil II (fat oil) by means of alkalis or by the enriching of certain fractions, are mixed and are heated with theexclusion of air for 24 to 48 hours with about 4 pounds of iron powder or iron oxid powder at 320 to 350 degrees C. under reflux or under pressure. The condensing reaction takes place with tli: tough, brownish black mass is obtained which is soluble in tar oils with a great increase of viscosity. Ten per cent. of the product heated for 24 hours at 350 C. under pressure is soluble in fat oil of a viscosity of about 19 degrees Engler 20 C.) and produces a lubricatin oil having a viscosity of about 45 degrees ng. (-l- 20 C.)

lVe claim 1. The process of manufacturing lubricating oils from coal tar oils or distillates of coal tar pitch embodying chiefly bases and phenols, consisting in'condensing and polymerizing the components of such substances by heat under pressure, and avoiding losses by evaporation during the heating of the substances.

2. The process of producing lubricants from coal tar oils or distillates of coal tar pitch, which consists in heating such product under reflux and preventing loss by evapo-- ration during the heating of the product.

3. The process of producing lubricants from coal tar oils or distillates of coal tar pitch which consists in heating such product under reflux in the presence of a catalyzer and preventing loss by evaporation during the heating of the product.

4. The process of producing lubricants from coal tar or distillates of coal tar pitch which consists in heating such product under reflux in the presence of iron oxid and preventing loss by evaporation during the heating of the product.

iron and preventing loss by evaporation during the heating of the product.

6. The process of producing lubricants from coal tar oils or distillates from coal tar pitch embodying chiefly bases and phenols, consisting in heating the components of the substance in an atmosphere of indifierent gases under pressure, and preventing loss by evaporation during the heating of the substance.

7. The process of producing lubricants from coal tar oil or distillates from coal tar pitch embodying chiefly bases and phenols consisting in heating the constituents of the material in an atmosphere of indifferent gases under pressure in the presence of a catalyzer and preventing loss by evaporation during the heating operation.

8. The process of producing lubricants fromjcoal tar oil or distillates from coal tar pitch embodying chiefly bases and phenols consisting in heating the constituents of the material in an atmosphere of indifferent gases under pressure in the presence of iron oxid and preventing loss by evaporation during the heating operation.

9. The process of producing lubricants from coal tar oil or distillates from coal tar pitch embodying chiefly bases and phenols consisting in heating the constituents of the material in an atmosphere of indifferent gases under pressure in the presenceof powdered oxid of iron and preventing loss by evaporation during the heating operation.

10. As anew article of manufacture, a lubricating oil consisting of condensed and polymerized coal tar oils or distillates from coal tar pitch having high viscosity and being soluble in tar oils, benzol, xylol, and mineral oils.

11. As a new article of manufacture, a lubricant consisting of condensed and polymerized bases and phenols and coal tar oils or distillates from coal tar pitch having high viscosity and being soluble in tar oils, benzol, xylol, and mineral oils.

In testimony whereof we have hereunto set our hands in presence of two subscribing witnesses.

HELMUT KLEVER. LUDWIG CARL LAU'lIlNSGHLXGER. OSWALD HELMUTH GOHRING. 

